RESUMO
Objective: To establish and determine the content of the genotoxic impurity piperidine in the active pharmaceutical ingredient (API) of rimonabant using a liquid chromatography-mass spectrometry (LC-MS) method. This study underscores the importance of detecting piperidine due to its potential health risks, including carcinogenic and mutagenic effects, thus highlighting the critical need for rigorous quality control in pharmaceutical products. Methods: An Atlantis C18 column (5 µm, 3.9×100 mm) was chosen for separation due to its high efficiency and selectivity for piperidine, with a gradient elution of 0.05% formic acid-water (A) and methanol (B) as the mobile phase at a flow rate of 1.0 mL/min. The column temperature was optimized at 30°C to ensure peak resolution and sensitivity, the injection volume was set to 5.0 µL to minimize sample consumption while maintaining detectability, and the analysis time was kept at 7 min for efficient throughput. Results: Piperidine demonstrated excellent linearity in the concentration range of 0.03-0.40 µg/mL (R>0.99), with a detection limit of 0.01010 µg/mL. This detection limit is significantly lower than regulatory thresholds, indicating the method's high sensitivity compared to existing methods and its adequacy for regulatory compliance in pharmaceutical quality control. Conclusion: This LC-MS method not only demonstrated high accuracy, good repeatability, and strong durability but also sets a benchmark for future research, regulatory practices, and pharmaceutical quality control. By accurately detecting low levels of genotoxic impurities like piperidine, this method supports the development of safer drug formulations and underscores the importance of stringent quality control measures in the pharmaceutical industry.
RESUMO
BACKGROUND: Some studies indicate unsafe injection practices, which are associated with the transmission of blood-borne pathogens, exist extensively, in the developing countries. AIMS: To investigate the status of injection services, knowledge and attitude of health workers with regard to injection practices at all levels of the health facilities in Jingzhou district of China; and to provide useful scientific data in order to formulate a feasible, standard measure on injection safety. SETTINGS: Four district health care facilities, 6 township health centers, 14 village clinics and 14 community health stations. DESIGN: A retrospective cross-sectional study. MATERIALS AND METHODS: By examining the medical records in 2004, observing injection practices and interviewing health workers, the quantitative and qualitative data were collected and analyzed. RESULTS: Out of 1,452 medical records sampled, 1,450 patients had received at least one injection in the period of hospitalization, with an injection rate of about 100% and an average of 10.9 injections per patient. The most frequent injected drug was antibiotic (48%, 7,674/15,857). The prescriptions of 5,655 outpatients were detected, with an injection rate of 52% (2,962). The field observation found that the proportion of unsafe injections was 16% (28/175) and that of unnecessary injections was 57% (99/175). Among 118 professional employees interviewed, those who knew that human immunodeficiency virus, hepatitis C virus and hepatitis B virus might be transmitted by the contaminated syringes and needles accounted for 95% (112), 59% (70) and 89% (105) respectively. CONCLUSIONS: Among the medical facilities of Jingzhou district, the injection rate was very high and the quality of injection practices should be further improved.
